EP3390284A1 - Methods for removing chloride from fertilizer wastewater - Google Patents
Methods for removing chloride from fertilizer wastewaterInfo
- Publication number
- EP3390284A1 EP3390284A1 EP16812951.8A EP16812951A EP3390284A1 EP 3390284 A1 EP3390284 A1 EP 3390284A1 EP 16812951 A EP16812951 A EP 16812951A EP 3390284 A1 EP3390284 A1 EP 3390284A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fertilizer plant
- wastewater
- chloride
- electrolyte
- fertilizer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003337 fertilizer Substances 0.000 title claims abstract description 79
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000002351 wastewater Substances 0.000 title claims abstract description 47
- 239000003792 electrolyte Substances 0.000 claims abstract description 62
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 29
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 28
- 239000011707 mineral Substances 0.000 claims abstract description 28
- 239000010842 industrial wastewater Substances 0.000 claims abstract description 10
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 230000003134 recirculating effect Effects 0.000 claims description 3
- 210000004027 cell Anatomy 0.000 description 42
- 230000008569 process Effects 0.000 description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 20
- 238000012546 transfer Methods 0.000 description 17
- 239000007789 gas Substances 0.000 description 15
- 235000010755 mineral Nutrition 0.000 description 13
- 239000012528 membrane Substances 0.000 description 12
- 239000000460 chlorine Substances 0.000 description 11
- 229910052801 chlorine Inorganic materials 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000003513 alkali Substances 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- -1 hydroxide ions Chemical class 0.000 description 6
- 239000002367 phosphate rock Substances 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 235000015097 nutrients Nutrition 0.000 description 5
- 238000001223 reverse osmosis Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000005201 scrubbing Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 238000010612 desalination reaction Methods 0.000 description 4
- 239000003651 drinking water Substances 0.000 description 4
- 235000020188 drinking water Nutrition 0.000 description 4
- 238000000909 electrodialysis Methods 0.000 description 4
- 239000002360 explosive Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000010405 anode material Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 238000005115 demineralization Methods 0.000 description 3
- 230000002328 demineralizing effect Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000619 316 stainless steel Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910000457 iridium oxide Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000007909 melt granulation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000003204 osmotic effect Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 229920002449 FKM Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 241001377938 Yara Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- YNGQHHUHCOYPKT-UHFFFAOYSA-L azanium;calcium;phosphate Chemical class [NH4+].[Ca+2].[O-]P([O-])([O-])=O YNGQHHUHCOYPKT-UHFFFAOYSA-L 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000008364 bulk solution Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Inorganic materials [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 229910001902 chlorine oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004807 desolvation Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- YNKVVRHAQCDJQM-UHFFFAOYSA-P diazanium dinitrate Chemical compound [NH4+].[NH4+].[O-][N+]([O-])=O.[O-][N+]([O-])=O YNKVVRHAQCDJQM-UHFFFAOYSA-P 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000003295 industrial effluent Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 235000021049 nutrient content Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical class [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002354 radioactive wastewater Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46123—Movable electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/4611—Fluid flow
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
- C02F2201/461—Electrolysis apparatus
- C02F2201/46105—Details relating to the electrolytic devices
- C02F2201/46115—Electrolytic cell with membranes or diaphragms
Definitions
- This invention relates to a novel system and method for removing chloride from fertilizer industrial wastewater and more particularly
- the goal is to reduce the amount of wastewater being discharged into the environment by recirculating the wastewater effluent back into the industrial system itself.
- the nature of the wastewater may vary depending on the type of fertilizer being produced and the specific processes involved.
- Mineral fertilisers contain one or more primary (major) nutrients nitrogen (N), phosphorus (P) or potassium (K) in inorganic form or as urea or cyanamide.
- the primary nutrients N, P and K are required by plants in large or moderate amounts.
- mineral fertilisers also contain other nutrients required by plants to a minor degree, such as Ca, Mg, and S. Trace elements required in small quantities are B, CI, Cu, Fe, Mn, Mo, Zn.
- Fertilizers are classified in terms of their major nutrient contents: straight fertilisers generally contain only one major or primary nutrient (N, P or K) whereas complex fertilizers contain two or more major nutrients ( NP, PK or NPK and more particularly NP or NPK fertilizers).
- the main effluent components in NP or NPK wastewater are ammonia, nitrate, fluoride and phosphate, and the wastewater may also contain heavy metals from the phosphate rock, such as Cd, Hg and Zn.
- chloride removal is not one of them. Effectively, chloride is not typically considered as an important contaminant in fertilizer wastewater. This may be due to the relative low levels of chloride seen in fertilizer wastewater which may only be on the order of 1000 ppm. For comparison, drinking water has maximum levels of 250 ppm, whereas salt water contains 35,000 ppm and brine has in excess of 50,000 ppm. As such, the levels seen in fertilizer wastewater are not generally considered to be an environmental concern.
- wastewater from a fertilizer plant is directed towards an electrochemical cell and chloride is removed by electrolysis.
- the fertilizer plant is a nitrophosphate fertilizer plant, meaning that the plant uses the nitrophosphate process to make fertilizers such as complex fertilizers.
- the wastewater may be from other mineral fertilizer or organo-mineral fertilizer processes.
- the fertilizer plant may produce compositions comprising ammonium nitrate.
- the fertilizer plant may produce compositions comprising ammonium nitrate by a melt granulation step.
- a fertilizer plant is any factory producing compositions that can be used as fertilizers, such as, without limitation ammonium nitrate.
- ammonium nitrate can be used as an explosive in addition to its use as a fertilizer. Accordingly, any plant manufacturing ammonium nitrate is considered to be a fertilizer plant regardless of the ultimate use of the ammonium nitrate.
- the chloride concentration may be reduced to levels lower than 500 ppm, more particularly 350 ppm or even more particularly lower than 250 ppm.
- electrochemical cell may be increased to make the electrochemical cell more efficient.
- mass transfer There are many ways of increasing the mass transfer including:
- the mass transfer is increased by electrolyte jetting.
- a fertilizer plant is fluidly connected to an electrochemical cell having an anode and a cathode such that wastewater from the fertilizer plant can be treated by the electrochemical cell to remove chloride.
- the fertilizer plant is a nitrophosphate, other mineral or organo-mineral fertilizer plant.
- the electrochemical cell may be fluidly connected to the fertilizer plant in such a way as to allow the wastewater to be recirculated back to the fertilizer plant.
- the electrochemical cell may further comprise electrolyte jets. When the electrolyte jets are located in the anode, the jets may improve the efficiency of the electrolysis by increasing mass transfer. When the jets are additionally located at the cathode, the jets may also be used to avoid high local pH and scaling of the cathode.
- electrolysis is used for the removal of chloride from industrial wastewater from an industrial fertilizer plant.
- the industrial fertilizer plant is a nitrophosphate, other mineral or organo-mineral fertilizer plant.
- Figure 1A is a side view of an electrochemical cell
- Figure IB is a cross- sectional view of one embodiment along axis A of Figure 1A
- Figure 1C is a cross-sectional view of an alternate embodiment along axis A of Figure 1A.
- Figure 2A is a front view of the electrochemical cell of Figures 1A and B;
- Figure 2B is a cross-sectional view along axis B of Figure 2A;
- Figure 2C is a cross-sectional view along axis C of Figure 2A.
- Figure 3 is a plot of chloride concentration over time during electrolysis of a sample of wastewater from a nitrophosphate fertilizer plant.
- Figure 4 is a plot of chloride concentration over time during electrolysis at three different current densities and with the use of electrolyte jetting.
- Figure 5 is a plot of chloride concentration over time after the electrolysis had been completed in a system with a lid (square) and in a system without a lid (triangle).
- Chloride can be seen in fertilizer wastewater, particularly wastewater from the nitrophosphate, other mineral or organo-mineral process.
- the chloride may have originated from the phosphate rock, depending on the source of phosphate rock. This impurity may be present in only modest concentrations on the order of 1000 ppm. If the wastewater is merely released into the environment, this level of chloride present may not present any environmental or regulatory concern. However, if the wastewater is then recirculated back into the fertilizer plant, then chloride when present even in modest amounts can destabilize ammonium nitrate which can become explosive and present a significant safety concern.
- Chloride has been identified in other industrial processes as a pollutant that can be removed though typically relatively high concentrations are seen before it is characterized as such. In these circumstances, chloride has been recognized as adding to the solids content and increasing the corrosive character of water. Alternatively, chloride is removed when the end result is drinking water which requires very low levels of chloride to be present, typically less than 250 ppm. Means of treatment are typically demineralization, reverse osmosis, electrodialysis, and evaporation (see Chapter 1 "Water Sources, Impurities and Chemistry", Handbook of Industrial Water Treatment, GE Power & Water,www.gewater.com/handbook/index.jsp, accessed 5 October 2015).
- Demineralized water is water that has had almost all of its mineral ions removed, such as cations like sodium, calcium, iron, and copper, and anions such as chloride, fluoride, nitrate, carbonate and sulphate.
- Demineralization is a chemical process that uses specially manufactured ion-exchange resins, which exchange hydrogen and hydroxide ions for dissolved minerals, and then recombine to form water. Because most non-particulate water impurities are dissolved salts, demineralization produces a high purity water that is generally similar to distilled water, and this process is quick and without scale buildup.
- Reverse osmosis involves forcing water through an osmotic membrane that rejects salts and allows water flux under pressures in excess of osmotic pressure.
- Reverse osmosis is currently the most widely practiced seawater desalination process and produces a permeate desalinated water that lacks ionic constituents and can be too pure for release into the environment.
- evaporation, or thermal desalination water is evaporated and condensed, sometimes in multiple stages, in order to recycle the latent heat of
- Electrochemically, electrodialysis is commonly practiced for desalination.
- salt ions are transferred across ion exchange membranes in a stack under the action of a galvanic potential.
- the galvanic potential is supplied as a voltage generated at an anode and cathode.
- the salt concentration of output product water from electrodialysis can be adjusted by adjusting the current applied to the stack.
- Salt ions are transferred from diluent or product chamber to concentrated saltwater in the concentrate chamber under a direct current electric field applied at the electrodes.
- a practical concentration factor of five to ten is common; that is, transferring ions from a diluent saltwater with a concentration of 2000 ppm to a concentrate saltwater with a concentration of between 10,000 ppm and 20,000 ppm.
- Electrolysis is an old technology dating to the 19 th century and still used in the chlor-alkali industry where sodium chloride is electrolyzed to produce the chemicals chlorine and sodium hydroxide (caustic soda). However, the process starts with brine, i.e. very high concentrations of sodium chloride on the order of 50,000 ppm. Such high concentrations allow efficient electrolysis.
- brine i.e. very high concentrations of sodium chloride on the order of 50,000 ppm.
- Such high concentrations allow efficient electrolysis.
- GB2499025 a process is described wherein aggressive decontaminating agents, such as HCI or NaCI, are used in the decommissioning of nuclear facilities.
- the UK patent application reports using electrolysis to remove chlorides from the radioactive wastewater. There is no discussion on why chloride is mentioned as a pollutant or any dangers associated therewith.
- electrolysis can be used to treat wastewater from fertilizer plants.
- electrolysis can actually be used at modest starting levels of chloride concentration of around 1000 ppm, much less than that seen in the chlor-alkali industry where chloride
- concentrations of 50,000 ppm are necessary for the efficient hydrolysis of chloride. Further, electrolysis can be used to bring the chloride concentration to levels lower than 500 ppm and more particularly lower than 350 ppm, and even more particularly lower than 250 ppm. As mentioned above, this ca n have particular advantages in relation to the nitrophosphate, other mineral or organo-minera l fertilizer processes, and even more particularly when the wastewater is recirculated back to the fertilizer plant.
- Electrolysis is a well-known technique and the following discussion on the reactions at the electrodes, as well as the nature of potential electrodes and electrolytes are not meant to limit the generality of the technique to the skilled person.
- Treatment of the effluent from the nitrophosphate, other mineral or organo-minera l fertilizer plant in the electrochemical cell facilitates the removal of chloride which is then liberated as chlorine gas.
- the chlorine gas may then be treated in an off-gas scrubber prior to release of any remaining harmless gases to the atmosphere.
- Suitable off-gas systems which may be used to scrub the liberated chlorine may, for example, use NaOH as the scrubbing agent. This would then produce NaCI and NaCIO, which may be re-used as a decontamination agent.
- solid state scrubbers can be employed.
- the cathode reaction involves the release of hydrogen gas, while oxygen and chlorine are evolved at the anode. It is generally beneficial to separate the anode and cathode reactions through the use of a separator or membrane (porous or ion selective). This may have multiple beneficial results including:
- the anolyte is the effluent from the fertilizer process, more particularly from the nitrophosphate, other mineral or organo-mineral process, referred to above as the fertilizer wastewater.
- the catholyte may also be the effluent from the wastewater or a concentrated salt solution, an acid solution such as nitric acid, water or another appropriate solution chosen by a skilled person. I n more particular embodiments, the catholyte is the wastewater from the fertilizer plant.
- the anode material of the cell should show stability in the electrolyte. I n addition, the material should be suitable for both oxygen and chlorine evolution and demonstrate low wear rates for both reactions, as well as low
- anode material should show higher overpotentials for other reactions, such as oxygen evolution.
- Typical materials for use as anode materials include boron-doped diamond, coated titanium (coated with oxides of metals, e.g. iridium oxide, mixed iridium/ruthenium oxide and tin oxide) and bulk platinum.
- electrodes known from the chlor-alkali industry can be used such as a DSATM electrode from Permascand.
- the selection of materials for the cathode materials is not as critical, with the main requirement being for stability in the electrolyte.
- stainless steel is particularly suitable, but this in no way limits the number of available materials, and a wide range of other materials which would be readily apparent to a person skilled in the art may also be employed for this purpose.
- Typical separators/membranes are polymeric in nature and may comprise any of a number of commercially available alternatives which would be apparent to a skilled person. Common examples include, for example, an asbestos diaphragm, a Nafion ® (sulphonated tetrafluoroethylene based fluoropolymer copolymer) cationic selective membrane or a microporous polyethylene separator.
- separators used in the chlor-alkali industry may be beneficially used.
- the membranes used in the chlor-alkali industry are commonly made of perfluorinated polymers. The membranes may have from one up to three layers, but generally consist of two layers.
- One of these layers consists of perfluorinated polymer with substituted carboxylic groups and is adjacent to the cathodic side.
- the other layer consists of perfluorinated polymer with substituted sulphonic groups and is adjacent to the anodic side.
- the membrane is generally reinforced with PTFE fibres.
- a suitable separator may be a PMX ® membrane from De Nora. At the anode, the reaction can be broken down into several discrete steps:
- the first step namely the mass transport is the limiting step. This is due to the relatively dilute chloride concentrations that are present which are typically on the order of only 1000 ppm.
- electrode/electrolyte the use of 3D electrodes, and the incorporation of inert mesh turbulence promoters.
- mass transfer may also be increased through the use of jets used to force the convection along the anode.
- the jet stream may be from a nozzle, such as a tube, or a hole or the like, directed at an angle, often perpendicularly to the surface of the anode.
- the mass transfer coefficient will be very high at the centre of the jet (also known as the stagnation point) and it decreases with increasing distance from the stagnation point.
- the jets may comprise standard pumps that direct anolyte through feed pipes with holes of the appropriate diameter. The orientation of the holes can then be adjusted to direct the flow of anolyte towards the anode.
- the jets may be located at the base of the electrochemical cell though a person skilled in the art would be able to optimize, through routine experimentation, the placement of the jets, the number of jets, the size of the holes, and the velocity of the resulting anolyte flow depending on the dimensions and orientation of the particular electrochemical cell.
- Jets can be easily adapted for many different electrochemical cells, both at the laboratory testing scale and in industrial use. It simply involves adjusting the stream velocity, orientation, and number of jets to be practicable for a large number of different sizes and orientations of electrochemical cells. This can be done without any inventive skill and involves merely routine optimization. This is in contrast to many of the other techniques where it may be necessary to use only specific sizes or orientations of the underlying electrochemical cell in order to efficiently increase the mass transfer. For example, ultrasound is mentioned often in the literature where the ultrasound causes the implosion of bubbles leading to shock waves and turbulence. However, this requires a relatively high power source that is located close to the electrodes making it practical for only relatively small cells only.
- Electrolyte jetting may also be used at the cathode to avoid high local pH and scaling of the cathode.
- electrolyte jets allows a much more efficient electrolysis and permits the chloride concentration to be reduced to below 500 ppm, more particularly below 350 ppm, below 300 ppm or below 250 ppm.
- the components of the cell, including the electrolytes and fluid circuits are adapted to handle the gas evolution, such that the evolved gases may be disengaged from the fluid streams and then suitably post-treated. Nevertheless, chlorine gas in particular is soluble in aqueous solutions. This can lead to the gas remaining in solution and potentially participating in back-reactions to regenerate chloride ion.
- hypochlorous acid HOCI
- Ammonium ion would also be expected in wastewater, particularly when the wastewater is NPK fertilizer wastewater.
- the hypochlorous acid may then react with the ammonium ion as follows:
- dissolved chlorine may then react to regenerate chloride within the wastewater.
- jets as discussed above aids in not only increasing the mass transfer but also in releasing the chlorine gas from solution and reducing the likelihood of the above back- reactions occurring. Nevertheless, some dissolved chlorine is expected to remain in solution.
- a desirable level of chloride may be less than 500 ppm and more particularly less than 350 ppm.
- Using the electrolyte jets allows the chloride concentration to be reduced to less than 250 ppm, or less than 200 ppm or even less than 150ppm and at this level, even if there is some back-reaction from dissolved chlorine to chloride ions, the resulting level of chloride ion present in solution would still be below the desired level of 500 ppm or 350 ppm.
- nitrophosphate fertilizer plant lower ultimate levels of chloride or chlorine that is obtained would be better. Nevertheless, for most practicable purposes a level of lower than 500, more particularly lower than 350 ppm would normally be considered acceptable.
- Figures 1 and 2 illustrate typical electrochemical cells.
- Figure 1A is a side view of an electrochemical cell 10 with an electrolyte inlet 20 and an electrolyte outlet 30.
- Figure IB is a cross- sectional view along axis A of Figure 1A with electrolyte jets 45 and separator 40.
- Electrolyte jets 45 may, for example, be holes in a metal tube extending from electrolyte inlet 20.
- a pump (not shown) may then be used to force the electrolyte through the holes in the electrolyte jets 45 with a particular velocity and orientation.
- the exact number of holes, the orientation, size and resulting velocity of the electrolyte jet stream can be easily optimized without any inventive skill and will depend on the size and dimensions of the particular electrolyte cell 10.
- Electrolyte may then recirculate from the electrolyte inlet 20, across the electrolyte cell 10 and exit through electrolyte outlet 30 to the pump and then back through electrolyte inlet 20. This recirculation may continue for the duration of the electrolysis.
- a second pump used to recirculate the catholyte separately would be beneficial to avoid any mixing of the gases evolving from the anode and cathode.
- the electrolysis could be done continuously.
- the duration of the electrolysis may be less than 24 hours, less than 5 hours, more particularly less than 4 hours, more particularly less than 3 hours, or less than 2 hours.
- the electrolysis is from as little as 5 minutes, for example from 5 minutes to 24 hours, from 5 minutes to 5 hours, 5 minutes to 4 hours, 5 minutes to 3 hours, 5 minutes to 2 hours, 5 minutes to 1 hour, 30 minutes to 5 hours, 30 minutes to 4 hours, 30 minutes to 3 hours, 30 minutes to 2 hours, 1-8 hours, 1-5 hours, 1-4 hours, 1-3 hours, or 1-2 hours.
- the time required relates to the electrode area and the volume fraction.
- Figure 1C is an alternate embodiment where additional metal tubes 50 extend perpendicularly from electrolyte jets 40 whereby additional holes in tubes 50 may be orientated to further increase mass transfer within the electrochemical cell 10.
- Figure 2A is a front view of the embodiment in Figure IB and shows electrochemical cell 10 with electrolyte inlet 20, electrolyte outlet 30, gas inlet 80 and gas outlet 90.
- Figure 2B is a cross-sectional view of Figure 2A across axis B and shows anode 60, separator 40 and cathode 70.
- Figure 2C is a cross- sectional view of Figure 2A across axis C and additionally shows electrolyte jets 45.
- An electrochemical cell was constructed with two non-polar anodes connected in parallel and three non-polar cathodes also connected in parallel.
- the anodes were made of 2.5 mm thick plates of DSA (Permascand, Sweden).
- the three cathodes were made of 3 mm stainless steel (316L).
- the electrolyte was an aqueous solution comprising 3.6 wt% dissolved NH 4 N03 and 1000 ppm CI " in the form of dissolved NH 4 CI.
- the pH was adjusted to 1.4 by addition of aqueous HNO3.
- the electrolyte was circulated by means of a pump.
- a separator was employed to avoid contact between the evolved gases, 0 2 , Cl 2 and H2.
- the separator was made of PTFE and treated with Membratex (Svenska Textilfilter) and it was 1.3 mm thick with a density of 750 kgm 3 .
- the hydrogen that evolved from the cathode was collected in a box placed at the top of the cathode, and the gas was dissipated into a ventilation hood about 2 m above the cell.
- the anode gases, 0 2 and Cl 2 were dissipated directly into the ventilation chamber.
- a chloride sensitive electrode (Radiometer Copenhagen) was used in the electrolyte to continuously measure chloride concentration. Operating conditions were held at ambient temperature with a pH of 1-1.4 at the anode and below 3.5 at the cathode.
- An electrochemical cell was equipped with an anode which was a dimensional stable anode from Permascand, and the cathode was SS 316 stainless steel.
- the membrane separator was a PMX ® membrane from De Nora. The pH of both the anode and cathode electrolytes were monitored
- a chloride sensitive electrode was used on the anode side to continuously measure chloride concentration.
- the electrolyte used was wastewater from Yara International in Porsgrunn and was representative of industrial wastewater from the nitrophosphate process to make a complex fertilizer.
- the anodic current density was 62 A m 2 .
- the electrochemical cell was further equipped with two pumps, one for the anolyte and another for the catholyte. The pumps were used with a feed pipe at the base of the electrochemical cell to create jets of electrolyte that were directed towards the respective electrodes.
- a schematic of the electrochemical cell is illustrated in Figures 1A and IB.
- the construction material of the cell was PVC.
- the main compartment was machined out of a 60 mm thick PVC block.
- the screws are made of 316 except for the screws fixing the anode that is made of PVC .
- the O-rings are made of Viton
- the anolyte and the catholyte was fed through the electrolyte inlets 20 shown at the bottom of the cell 10, and further into electrolyte jets 45 equipped with jets (see figure IB).
- the jets were simply holes in a metal tube with a diameter of 2 mm (four holes in each inlet tube).
- the electrolyte was further flowed through the electrolyte outlet 30 and into a small reservoir with CI " selective electrode and pH electrode (not shown).
- the electrolyte was then going to a pump (not shown) and pumped back into the electrolyte cell 10.
- the normal flow rate was about 50 I h "1 , equivalent to a fluid speed out of the jets of approximately 2.2 m s "1 .
- the separator 40 was placed on a 20 mm wide terrace machined out in the PVC and fixed with a 5 mm thick PVC frame. This frame separates the gasses from the anode and the cathode. Both the electrodes are screwed to the inner wall of the cell, and a current collector goes through the cell wall equipped with an O-ring seal.
- the additional jets directed towards the cathodes were used to avoid high local pH and reduce any cathode scaling.
- Figure 3 illustrates three typical experiments where the chloride concentration was measured at different currents. Run A was at 5 A; run B was at 10 A; and run C was at 20 A. A current of 10 A is equivalent to 120 Am 2 .
- Figure 3 shows a significant improvement for chloride removal compared to the cell presented in Example 1. The figure also shows that the rate of chloride removal increased with increasing current and that this rate decreased with chloride concentration. Calculations showed that the Faradaic current efficiency was about 9 % for chloride removal for all the experiments presented in Figure 2.
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EP3623347A1 (en) * | 2018-09-17 | 2020-03-18 | Yara International ASA | Method for removing a contaminant from wastewater from an industrial plant and a system for performing such method |
WO2023147290A2 (en) * | 2022-01-25 | 2023-08-03 | Georgia Tech Research Corporation | Salinity exchange for low-cost and high-quality potable water |
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